CN1651514A - Fibrous polyaniline / diatomite nano-conductive composite material - Google Patents
Fibrous polyaniline / diatomite nano-conductive composite material Download PDFInfo
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- CN1651514A CN1651514A CN 200510023159 CN200510023159A CN1651514A CN 1651514 A CN1651514 A CN 1651514A CN 200510023159 CN200510023159 CN 200510023159 CN 200510023159 A CN200510023159 A CN 200510023159A CN 1651514 A CN1651514 A CN 1651514A
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- composite material
- diatomite
- polyaniline
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- oxygenant
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Abstract
An electrically conductive fibrous polyphenylamine/diatomite nano-compound is prepared from phenylamine, diatomite, hypochlorite and the aqueous solution of inorganic acid through one-step in-situ oxidizing-polymerizing reaction. Said nano-compound features higher thermal stability and electric conductivity.
Description
Technical field
The present invention relates to a kind of conducing composite material, specifically, relate to a kind of polyaniline/diatomite nano-conductive composite material.
Background technology
(chemical ingredients mainly is SiO to diatomite
2.nH
2O) belong to nonmetalliferous ore, characteristics such as it has that look shallow, light weight, voidage is big, adsorptivity is strong, heat insulation, sound insulation, insulation, fusing point height, Heat stability is good, the more important thing is cheaply, thereby be widely used in and produce flocculating aids, filler, sorbent material, abrasive material and carrier or the like.
Filler is diatomaceous second largest purposes.And as filler, a diatomaceous important use is: be used for natural rubber, elastomeric reinforcing filler, especially in free of contamination light-colour rubber goods, diatomite can substitute the white carbon black of reinforcement, or part substitutes white carbon black.Although diatomite has many good qualities as filler, diatomite is isolator.Along with the continuous development of electronic industry, people are just growing to the demand of rubber with antistatic property and plastics, and therefore the exploitation diatomaceous earth filler that has reinforcement and conductivity concurrently will have more wide application prospect.
Conductive polymers is nearly type material that grew up in two, 30 years.Because therefore the physical and chemical performance that conductive polymers has a series of uniquenesses can be widely used in multiple functional material of exploitation and device.In recent years, be that the main functions matrix material has been subjected to chemistry and extensive concern and research, the especially electrically conductive polyaniline of material educational circles and the matrix material of many inorganic materials with the conductive polymers.Although polyaniline is cheap, environmental stability is good, electrically conductive polyaniline is indissoluble, infusible, and this has just greatly limited its application.Domestic and international many scholars' result of study shows that mixing by organic acid to solve the solubility problem of electrically conductive polyaniline in some common organic solvents to a certain extent, but the pollution that a large amount of organic solvent that uses has brought environment.The another kind of approach that solves the electrically conductive polyaniline workability is the matrix material that directly prepares electrically conductive polyaniline and other material by in-situ oxidizing-polymerizing.Also be a lot of by the polyaniline of in-situ oxidizing-polymerizing method preparation and the matrix material of other inorganic materials at present, the inventor also once by polyaniline to diatomaceous prepared by surface modification the polyaniline/diatomite conducing composite material, have the circular or oval-shaped algae lobe of micropore but the pattern of resulting conduction diatomite composite material still is a diatomite.Up to now, the achievement in research for preparing fibrous polyaniline/diatomite nano-conductive composite material by a step in-situ oxidizing-polymerizing method does not still have open report.
Summary of the invention
The object of the invention is, a kind of fibrous polyaniline/diatomite nano-conductive composite material that passes through step in-situ oxidizing-polymerizing method preparation is provided, and fills up blank of the prior art.
Fibrous polyaniline/diatomite nano-conductive composite material of the present invention, it is characterized in that, described conducing composite material is that raw material, chlorite are that oxygenant, inorganic acid aqueous solution are solvent with aniline monomer and diatomite, makes through a step in-situ oxidizing-polymerizing;
Wherein: aniline monomer and diatomaceous weight ratio are 1: 0.5～3.0, and the mol ratio of oxygenant and aniline monomer is 1: 0.8～3.0.
Fibrous polyaniline/diatomite nano-conductive composite material of the present invention, its Fibre diameter are less than 100nm, and electric conductivity is 0.01～5S/cm.
In the present invention, preferred solvent is hydrochloric acid or sulfuric acid; Preferred oxygenant Textone; The in-situ oxidizing-polymerizing time of recommending is 2～12 hours.
Description of drawings
The diatomaceous transmission electron microscope picture of Fig. 1
The transmission electron microscope picture of Fig. 2 fibrous polyaniline/diatomite nano-conductive composite material
Embodiment
Preparing fibrous polyaniline/diatomite nano-conductive composite material of the present invention comprises the steps:
(1) diatomite is ground to form 300 purpose particles, and ultrasonic cleaning 1～2 hour in dilute hydrochloric acid, it is dry under 50 ℃～100 ℃ conditions to filter the back.
(2) diatomite that will handle through step (1) and hydrochloric acid or aqueous sulfuric acid place reactor, in reactor, add a certain amount of aniline monomer (aniline monomer and diatomaceous weight ratio are 1: 0.5～3.0) again, behind ultra-sonic dispersion, add chlorite (mol ratio of chlorite and aniline monomer is 1: 0.8～3.0), oxypolymerization is 2～12 hours under agitation condition, filter, the vacuum-drying 24 hours under 50 ℃ of conditions of washing back, obtain target compound.
Fibrous polyaniline/diatomite nano-conductive composite material of the present invention not only has small-size effect, surface and the interfacial effect and the quantum size effect of nano material, and compare with existing polyaniline/diatomite conducing composite material (making by polyaniline finishing diatomite), have better thermostability and electroconductibility.
The present invention is further elaborated below in conjunction with embodiment, and its purpose only is better to understand content of the present invention and unrestricted protection scope of the present invention.
Embodiment 1
Get diatomite and the distilled aniline of 1.0g that 1.0g handled and put into the there-necked flask that contains 20ml 2M HCl solution, ultra-sonic dispersion adds the aqueous solution that 20ml contains 1.2g Textone oxygenant after 1 hour.Room temperature oxypolymerization is 5 hours under agitation condition, filters, washing back under 50 ℃ of conditions dry 24 hours, obtains jade-green pressed powder.The fiber diameter of prepared polyaniline/diatomite nano-conductive composite material is approximately 50～100nm, and specific conductivity is 1.5S/cm.
Embodiment 2
Get diatomite and the distilled aniline of 0.6g that 1.0g handled and put into the there-necked flask that contains 20ml 2M HCl solution, ultra-sonic dispersion adds the aqueous solution that 20ml contains 0.72g Textone oxygenant after 1 hour.Room temperature oxypolymerization is 2 hours under agitation condition, filters, washing back under 50 ℃ of conditions dry 24 hours, obtains jade-green pressed powder.The fiber diameter of prepared polyaniline/diatomite nano-conductive composite material is 50～100nm, and specific conductivity is 2.8 * 10
-2S/cm.
Embodiment 3
Get diatomite and the distilled aniline of 3.0g that 1.0g handled and put into the there-necked flask that contains 20ml 2M HCl solution, ultra-sonic dispersion adds the aqueous solution that 20ml contains 3.6g Textone oxygenant after 1 hour.Room temperature oxypolymerization is 5 hours under agitation condition, filters, washing back under 50 ℃ of conditions dry 24 hours, obtains jade-green pressed powder.The fiber diameter of prepared polyaniline/diatomite nano-conductive composite material is approximately 50～100nm, and specific conductivity is 3.6S/cm.
Embodiment 4
Get diatomite and the distilled aniline of 1.0g that 1.0g handled and put into the there-necked flask that contains 20ml 2M HCl solution, ultra-sonic dispersion adds the aqueous solution that 20ml contains 0.8g Textone oxygenant after 1 hour.Room temperature oxypolymerization is 5 hours under agitation condition, filters, washing back under 50 ℃ of conditions dry 24 hours, obtains jade-green pressed powder.The fiber diameter of prepared polyaniline/diatomite nano-conductive composite material is approximately 50～100nm, and specific conductivity is 0.6S/cm.
Embodiment 5
Get diatomite and the distilled aniline of 1.0g that 1.0g handled and put into the there-necked flask that contains 20ml 2M HCl solution, ultra-sonic dispersion adds the aqueous solution that 20ml contains 2.9g Textone oxygenant after 1 hour.Room temperature oxypolymerization is 5 hours under agitation condition, filters, washing back under 50 ℃ of conditions dry 24 hours, obtains jade-green pressed powder.The fiber diameter of prepared polyaniline/diatomite nano-conductive composite material is approximately 50～100nm, and specific conductivity is 1.2 * 10
-1S/cm.
Embodiment 6
Get diatomite and the distilled aniline of 1.0g that 1.0g handled and put into the there-necked flask that contains 20ml 2M HCl solution, ultra-sonic dispersion adds the aqueous solution that 20ml contains 1.4g potassium chlorite oxygenant after 2 hours.Room temperature oxypolymerization is 3 hours under agitation condition, filters, washing back under 50 ℃ of conditions dry 24 hours, obtains jade-green pressed powder.The fiber diameter of prepared polyaniline/diatomite nano-conductive composite material is 50～100nm, and specific conductivity is 7.2 * 10
-2S/cm.
Embodiment 7
Get the distilled aniline of 1.0g diatomite and 1.0g and put into the there-necked flask that contains 20ml 2M HCl solution, ultra-sonic dispersion adds the aqueous solution that 20ml contains 1.2g Textone oxygenant after 1 hour.Room temperature oxypolymerization is 12 hours under agitation condition, filters, washing back under 50 ℃ of conditions dry 24 hours, obtains jade-green pressed powder.The fiber diameter of prepared polyaniline/diatomite nano-conductive composite material is approximately 50～100nm, and specific conductivity is 1.1S/cm.
Embodiment 8
Getting diatomite that 1.0g handled and the distilled aniline of 1.0g puts into and contains 20ml 1M H
2SO
4In the there-necked flask of solution, ultra-sonic dispersion adds the aqueous solution that 20ml contains 1.2g Textone oxygenant after 1 hour.Room temperature oxypolymerization is 5 hours under agitation condition, filters, washing back under 50 ℃ of conditions dry 24 hours, obtains jade-green pressed powder.The fiber diameter of prepared polyaniline/diatomite nano-conductive composite material is 50～100nm, and specific conductivity is 2.9 * 10
-1S/cm.
Embodiment 9
Getting the distilled aniline of 1.0g diatomite and 1.0g puts into and contains 20ml 1M H
2SO
4In the there-necked flask of solution, ultra-sonic dispersion adds the aqueous solution that 20ml contains 1.2.g Textone oxygenant after 2 hours.Room temperature oxypolymerization is 5 hours under agitation condition, filters, washing back under 50 ℃ of conditions dry 24 hours, obtains jade-green pressed powder.The fiber diameter of prepared polyaniline/diatomite nano-conductive composite material is 50～100nm, and specific conductivity is 8.1 * 10
-1S/cm.
Claims (5)
1, a kind of fibrous polyaniline/diatomite nano-conductive composite material is characterized in that, described conducing composite material is that raw material, chlorite are that oxygenant, inorganic acid aqueous solution are solvent with aniline monomer and diatomite, makes through a step in-situ oxidizing-polymerizing;
Wherein: aniline monomer and diatomaceous weight ratio are 1: 0.5～3.0; The mol ratio of oxygenant and aniline monomer is 1: 0.8～3.0.
2, conducing composite material as claimed in claim 1 is characterized in that, wherein said oxygenant is Textone or potassium chlorite.
3, conducing composite material as claimed in claim 1 is characterized in that, wherein the in-situ oxidizing-polymerizing reaction times is 2～12 hours.
4, as any one conducing composite material as described in the claim 1～3, it is characterized in that wherein said mineral acid is hydrochloric acid or sulfuric acid.
5, conducing composite material as claimed in claim 4 is characterized in that, wherein used diatomite is through pre-treatment, that is: through grinding to form 300 purpose particles, and ultrasonic cleaning 1～2 hour in dilute hydrochloric acid, it is dry under 50 ℃～100 ℃ conditions to filter the back.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100231596A CN100365045C (en) | 2005-01-07 | 2005-01-07 | Fibrous polyaniline / diatomite nano-conductive composite material |
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| CNB2005100231596A CN100365045C (en) | 2005-01-07 | 2005-01-07 | Fibrous polyaniline / diatomite nano-conductive composite material |
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| CN1651514A true CN1651514A (en) | 2005-08-10 |
| CN100365045C CN100365045C (en) | 2008-01-30 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI508996B (en) * | 2013-08-14 | 2015-11-21 | Far Eastern New Century Corp | To reduce the color difference with the composition and conjugate polymer guide The method of forming an insulating region and a conductive region by a film and reducing the color difference between the regions |
| CN110204703A (en) * | 2019-04-26 | 2019-09-06 | 广东工业大学 | A kind of diatomite based composites and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102074279B (en) * | 2010-12-30 | 2012-05-23 | 北京工业大学 | Preparation method of multihole-structure-characterized conducting diatomaceous earth |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU551861A1 (en) * | 1974-08-15 | 1977-09-05 | Предприятие П/Я А-7629 | Method of preparing analine |
| CN1096487C (en) * | 1999-07-12 | 2002-12-18 | 武汉工业大学 | nm-class composite polyphenylamine-Fe2O3 material and its preparing process |
-
2005
- 2005-01-07 CN CNB2005100231596A patent/CN100365045C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI508996B (en) * | 2013-08-14 | 2015-11-21 | Far Eastern New Century Corp | To reduce the color difference with the composition and conjugate polymer guide The method of forming an insulating region and a conductive region by a film and reducing the color difference between the regions |
| CN110204703A (en) * | 2019-04-26 | 2019-09-06 | 广东工业大学 | A kind of diatomite based composites and preparation method thereof |
| CN110204703B (en) * | 2019-04-26 | 2021-10-19 | 广东工业大学 | Diatomite-based composite material and preparation method thereof |
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